聚苯胺/Fe3O4复合吸波材料的制备及表征

用原位聚合法合成了聚苯胺／Fe3O4（PANI/Fe3O4）复合材料,合成产物为以Fe3O4为核,聚苯胺为壳的球状微粒。采用FT-IR、XRD、XPS、TEM等方法对PANI/ Fe3O4进行了结构表征。以矩形波导法测定了PANI/Fe3O4在9．3GHz微波环境中的性能。结果表明,改变Fe3O4含量可以调节复合材料的电磁参数。当Fe3O4质量分数为10％时,复合材料介电损耗tgδε=1．87、磁损耗tgδμ=0．035,达到最大微波损耗7．641（-dB）,具有良好的吸波性能。     

Template synthesis and magnetic response of polyaniline/Fe3O4 composite microtubes

Template synthesis technique was employed to prepare magnetic polyaniline (PANI)/Fe₃O₄ composite microtubes using anodic aluminum oxide (AAO) membrane as template. Magnetic microtubes were obtained through in situ polymerization of aniline in the presence of Fe₃O₄ nanoparticles in the microchannels of template. A tubular structure was formed once when aniline was preferentially adsorbed and polymerized on the surface of channels wall. Electron microscope images demonstrated that the shape and size of guest (PANI/Fe₃O₄ composite microtubes) were strictly depended on those of the host (template channels). Magnetic force microscopy images showed that the PANI/Fe₃O₄ composite microtubes possessed reasonable magnetism and the magnetism distribution of microtubes was regular as distribution of template channels. Moreover, the magnetic response and oriented arrangement of PANI/Fe₃O₄ microtubes were fulfilled in the magnetic field. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Preparation and property characterization of PAA/Fe3O4 nanocomposite

PAA/Fe₃O₄ nanocomposites were prepared by mixing nano-Fe₃O₄ and polyacrylic acid (PAA) ethanol solution and then evaporating the solvent. The materials were characterized by transmission electron microscope (TEM), Fourier transform infrared spectroscope (FTIR), thermogravimetry analysis (TGA), dynamic ultra-micro hardness tester (DUMHT) and superconducting quantum interference device (SQUID) magnetometer. Results showed that PAA coordinated with nano-Fe₃O₄ to form a cross-linking structure. The presence of nano-Fe₃O₄ enhanced the thermal stability of the nanocomposite. The elasticity and hardness of the nanocomposite increased, and the indentation depth reduced with the increase of Fe₃O₄ content in the composites. The nanocomposites showed superparamagnetic properties at 300 K. Translated from Acta Scientiarum Naturalium Universitatis Sunyatseni, 2006, 45(5): 47–50 [译自: 中山大学学报 (自然科学版)]     

Hollow polyaniline/Fe3O4 microsphere composites: Preparation,characterization, and applications in microwave absorption

Hollow polyaniline/Fe₃O₄ microsphere composites with electromagnetic properties were successfully prepared by decorating the surface of hollow polyaniline/sulfonated polystyrene microspheres with various amounts of Fe₃O₄ magnetic nanoparticles using sulfonated polystyrene (SPS) as hard templates and then removing the templates with tetrahydrofuran (THF). The synthesized hollow microsphere composites were characterized by FT-IR, UV/Vis spectrophotometry, SEM, XRD, elemental analysis, TGA, and measurement of their magnetic parameters. Experimental results indicated that the microspheres were well-defined in size (1.50–1.80 μm) and shape, and that they were superparamagnetic with maximum saturation magnetization values of 3.88 emu/g with a 12.37 wt% content of Fe₃O₄ magnetic nanoparticles. Measurements of the electromagnetic parameters of the samples showed that the maximum bandwidth was 8.0 GHz over ?10 dB of reflection loss in the 2–18 GHz range when the Fe₃O₄ content in the hollow polyaniline/Fe₃O₄ microsphere composites was 7.33 wt%.     

Recent advances in the development OF Fe3O4-BASED microwave absorbing materials

Electromagnetic pollution has become a serious concern with the immense utilization of wireless information technologies and this has aroused huge interest in the area of microwave absorption. To solve this issue, fabrication of advanced, novel and superior microwave absorbing materials (MAM) with high electromagnetic wave absorption, wide absorption bandwidth, lightweight and cost-efficient are highly required. To date, magnetite (Fe₃O₄) is being thoroughly investigated as MAM, due to its exceptional dual electromagnetic properties (permittivity and permeability), proper saturation magnetization and high Curie temperature. However, large density and impedance mismatch are some of the limiting factors that hinder its microwave absorption performance (MAP). To circumvent these challenges, reduction of size to the nanoscale, fabrication of hierarchical nanostructures and/or conjugation with other lossy materials have been extensively explored as viable solutions to optimize the MAP of Fe₃O₄. In this review, the progressive research in the fabrication of Fe₃O₄ based nanocomposites as MAM is discussed. The factors influencing the MAP of these absorptive materials are likewise discussed in detail. Conclusively, some challenges, limitations, and future prospects in the development of Fe₃O₄ based MAM are put forth.     

Preparation of pod-like 3D Ni0.33Co0.67Fe2O4@rGO composites and their microwave absorbing properties

The ferrite/reduced graphene oxide (rGO) composites have attracted increasing attention due to the combination of the dielectric loss of rGO and the magnetic loss of ferrites. In this paper, pod-like 3D Ni_0.33Co_0.67Fe₂O₄@rGO composites were prepared using a solvothermal reaction followed by cold quenching. The structures and morphologies of as obtained composites were characterized using X-ray diffractometer, Raman microscope, photoelectron spectroscopy, scanning electron microscope and transmission electron microscope. The Ni_0.33Co_0.67Fe₂O₄ microspheres with a diameter of 100–150?nm were wrapped in rGO rolls due to the shrinkage of rGO in liquid nitrogen. The rGO sheets with ferrite microspheres wrapped in form the pod-like 3D network morphology. The minimum reflection loss of as-prepared composites reaches ?47.5?dB and the absorption bandwidth (RL<?10?dB) is 5.02?GHz. The composites show much better absorbing performances than pure Ni_0.33Co_0.67Fe₂O₄ microspheres and Ni_0.33Co_0.67Fe₂O₄-rGO mixture formed by mechanically blending of cold quenched pure rGO and ferrite microspheres.     

导电聚苯胺/泡沫玻璃复合吸波材料

以硼玻璃粉为原料，炭黑为发泡剂，三氧化二铁为添加剂，制备得到泡沫玻璃基体。再以苯胺(An)为单体，过硫酸铵(APS)为引发剂，通过原位聚合法和乳液聚合法制备了导电聚苯胺/泡沫玻璃复合材料。采用FTIR、XRD和SEM对泡沫玻璃和复合材料的形貌、结构进行了表征，矢量网格分析仪测量了材料的电磁参数，并模拟计算了材料的反射损耗。结果表明，当炭黑含量为0.03wt%，炭黑和三氧化二铁的摩尔比为3：2时，制备的泡沫玻璃气孔尺寸在1mm-1.2mm，抗压强度在1.7MPa-2.45MPa。电磁参数测试和反射损耗的结果表明，当聚苯胺的浓度为0.1mol/l时，复合材料的吸波性能最好。原位聚合所得复合材料最小反射损耗为-12.56dB，有效带宽为2GHz（8.2GHz-10.2GHz）。乳液聚合所得材料最小反射损耗为-13.38dB，有效带宽为2.2GHz（8.2GHz-10.4GHz）。     

GO/Fe_3O_4/ZnO的制备及其光助Fenton降解苯酚

采用水热法制备了GO/Fe_3O_4/ZnO复合材料,并用SEM、FT-IR、XRD等手段对其进行了表征。以苯酚为降解目标,探讨了GO/Fe_3O_4/ZnO复合材料用量、H_2O_2投加量、苯酚浓度和pH等因素对降解苯酚效果的影响。实验结果表明,在GO/Fe_3O_4/ZnO投加量为200 mg/L,H_2O_2投加量为12 mmol/L,pH=7.2的条件下,利用该复合材料对苯酚质量浓度为88.85 mg/L的油田污水进行光催化Fenton降解,60 min后,苯酚降解率可达98%。     

MoO3/g-C3N4复合材料的制备及光催化性能

以三聚氰胺和四水合钼酸铵为前驱体,采用水热法制备了MoO₃/g-C₃N₄复合光催化剂。利用X-射线衍射仪（XRD）、红外光谱仪（FT-IR）、扫描电子显微镜（SEM）、X射线光电子能谱仪（XPS）及紫外-可见漫反射仪（DRS）等对制备的样品进行了表征。表征结果显示,棒状的三氧化钼负载在层状C₃N₄表面,复合材料的光吸收能力有一定的增强。材料可见光催化降解亚甲基蓝（MB）溶液的实验表明,三氧化钼和g-C₃N₄所复合产生的异质结具有较好的吸收光强度及催化降解性能,尤其是5%（质量分数）MoO₃/g-C₃N₄复合材料光催化降解率最好,达到95.7%,高于纯三氧化钼和g-C₃N₄。自由基与空穴捕获实验表明,·O₂^-是光催化反应中的主要活性物种。MoO₃/g-C₃N₄复合材料在4个循环周期内表现出了优异的稳定性。     

氢氛还原法制备氧化铁/膨润土 复合材料及其表征研究

以膨润土和硝酸铁为原料,采用氢氛还原法制备Fe₃O₄/膨润土复合材料,并采用X射线衍射（XRD）、扫描电子显微镜（SEM）和电子能谱（EDS）做表征分析。通过实验得到最佳的工艺条件：n（OH^-）∶n（Fe³⁺）=1∶1、铁土比为10 mmol/g、还原温度为200 ℃、还原时间为30 min。制备的Fe₃O₄/膨润土具有良好的类Fenton催化性能、稳定性与磁分离性能。制备过程中铁元素化合物能够有效固载在膨润土上,并在氢气还原作用下转化为Fe3O4,所得Fe3O4/膨润土是结构分散、孔隙明显、物化形态优良的催化复合材料。     

Preparation of Fe3O4 particles from copper/iron ore cinder and their microwave absorption properties

In this study, magnetic Fe₃O₄ particles were prepared from copper/iron ore cider by precipitation oxidization method. The yield of Fe was 82.6 at%. XRD, TEM, SEM, EDS and microwave network analyzer were used to characterize the particles. The results showed that Fe₃O₄ particles were well crystallized and possessed an octahedral morphology, and the crystal size was about 200 nm; the sample with 70 wt% Fe₃O₄ exhibited the optimal absorbing ability, the minimum reflection loss was ?42.7 dB at 14.08 GHz and the bandwidth less than ?10 dB was about 4.2 GHz when the sample thickness was 1.9 mm. It was clearly demonstrated that the Fe₃O₄ particles prepared from copper/iron ore cider could be used as an effective microwave absorbing material.     

聚苯胺/氧化锌复合膜的制备及其防腐性能

将化学氧化法制备的聚苯胺(PANi)粉末溶于氮甲基吡咯烷酮溶剂后涂覆到制备有ZnO底层的碳钢基体上,获得了PANi/ZnO复合膜。通过扫描电镜、X射线衍射、极化曲线、电化学阻抗谱等测试手段分析了PANi/ZnO复合膜的形貌、成分、与基体的粘附力强度及在3.5%NaCl溶液中的耐腐蚀性能。结果表明,在碳钢基体上制备的PANi/ZnO复合膜中的ZnO呈纳米棒状,提高了复合膜的均匀性和表面平整性,增强了复合膜与金属基体的粘附力。与裸碳钢片相比,有复合膜层的试样的开路电位正向偏移180mV左右,自腐蚀电流密度降低。PANi/ZnO复合膜有效提高了碳钢基体的防腐性能。     

Effect of Fe3O4 concentration on 3D gel-printed Fe3O4/CaSiO3 composite scaffolds for bone engineering

In this study, porous calcium silicate (CaSiO₃) scaffolds were prepared by 3D gel-printing (3DGP) method and Fe₃O₄ water-based magnetic fluids (WMFs) were prepared by phacoemulsification compound chemical coprecipitation method. Fe₃O₄ WMFs were coated on CaSiO₃ scaffolds surface to prepare Fe₃O₄/CaSiO₃ composite scaffolds. The effect of WMFs with different Fe₃O₄ concentrations on porous CaSiO₃ scaffolds was studied. The composition and morphological characteristics of porous scaffolds were analyzed by using scanning electron microscope (SEM) and energy dispersive spectrometer (EDS) analysis. The magnetic properties were tested by vibrating sample magnetometer (VSM). The stability of Fe₃O₄ WMFs coatings and the degradability of composite scaffolds were tested by immersing them in simulated body fluid (SBF). The results show that when Fe₃O₄ concentration was 5.4% (w/v), the composite scaffolds had the highest saturation magnetization of 69.6 emu/g and the best stability in dynamic SBF. It is obviously that Fe₃O₄ WMFs coatings can be used for bone tissue engineering scaffolds repairing.     

Microwave absorption property of polyaniline nanocomposites containing TiO2 and Fe3O4 nanoparticles after FeCl36H2O treatment

It is important to manipulate the synthesis parameters or additives used in order to produce conducting polymer such as polyaniline (PAni) with moderate conductivity, magnetic and dielectric properties that could enhance its microwave absorbing and shielding properties. In this communication, novel PAni/HA/TiO₂/Fe₃O₄ nanomaterials with different Fe₃O₄ contents were prepared by template‐free method by using TiO₂ and Fe₃O₄ nanoparticles as dielectric filler and magnetic filler, respectively. Before addition of ammonium peroxydisulfate (APS) for polymerization, Fe₃O₄ aqueous solution was treated with FeCl₃6H₂O in order to disperse well the Fe₃O₄ in the mixture. The result shows that better dispersion of Fe₃O₄ in the mixture by FeCl₃6H₂O treatment could significantly improve the conductivity of the nanocomposites and also activate the formation of nanorods/tubes. Moreover, PAni/HA/TiO₂/Fe₃O₄ nanocomposites treated with FeCl₃6H₂O show better microwave absorption (99.950–99.999% absorption) compared with PAni/HA/TiO₂/Fe₃O₄ micro/nanocomposites (67.0− 99.4% absorption) without treatment in frequency range of 10–13 GHz. Among the prepared PAni/HA/TiO₂/Fe₃O₄ micro/nanocomposites and nanocomposites, PAni/HA/TiO₂/Fe₃O₄ nanocomposite (treated with FeCl₃6H₂O) with 40% Fe₃O₄ exhibit the best microwave absorption (99.999% absorption at 10 GHz) because of its high conductivity, high heterogeneity and moderate magnetization. POLYM. COMPOS., 2010. © 2010 Society of Plastics Engineers     

聚苯胺/四氧化三铁吸波材料的制备与性能

利用γ-氨丙基三乙氧基硅烷(KH550)氨基化改性Fe_3O_4纳米粒子,并以其为稳定剂、甲苯为软模板,与苯胺形成Pickering乳液,再以过硫酸铵(APS)为引发剂、HCl为掺杂剂,用界面聚合法合成了掺杂态聚苯胺(PANI)/KH550-Fe_3O_4复合材料。采用FTIR、SEM、XRD对样品形貌和结构进行了表征,通过振动样品磁强计(VSM)考察了不同浓度HCl对复合材料磁性能的影响。结果表明:当c(HCl)=0.1 mol/L时,复合材料的饱和磁强度高达24 841 A/m。用矢量网络分析仪(VNA)对复合材料的屏蔽和吸波性能进行了分析,结果表明:在c(HCl)=0.1 mol/L、复合材料厚度为1 mm、电磁波的频率为10 160 Hz下,复合材料的屏蔽效能高达40.682 dB,在12 400 Hz时反射损耗达-47.043 dB。     

Au/Fe3O4纳米复合材料的制备及其催化性能

通过将金纳米粒子铆接到Fe3O4载体表面,制得了Au/Fe3O4纳米复合粒子。首先以对苯二酚为还原剂还原HAuCl4制得球形金纳米粒子;然后采用溶剂热法制备Fe3O4磁性纳米颗粒,并用巯基丙酸(MPA)对其修饰;最后通过MPA与金纳米粒子之间的相互作用,将金纳米颗粒固定到Fe3O4表面。采用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X射线衍射仪(XRD)、傅里叶变换红外光谱仪(FTIR)和振动样品磁强计(VSM)和紫外-可见分光光度计(UV-vis)对所制备材料进行形貌、晶型、磁性和催化性能的表征。结果表明,金纳米颗粒成功包覆在Fe3O4表面,所得到的Au/Fe3O4复合纳米材料具有单分散性和超顺磁性,并且对NaBH4还原对硝基苯酚(4-NP)制备对氨基苯酚(4-AP)的反应显示出优良的催化性能。     

多孔Al2O3/SiC、MoSi2/SiC复合材料的制备及吸波性能

以Si、Al₂O₃、MoSi₂微粉和生物竹材为原料,采用包埋烧结法分别制备出SiC多孔材料、Al₂O₃/SiC、MoSi₂/SiC复合材料。采用XRD、SEM及波导法测试其物相组成、显微结构及吸波性能。结果表明：MoSi₂/SiC复合材料的厚度为2 mm时有明显的吸波特性,有效吸收带宽在X波段的9.65~12.4 GHz频率范围内达2.75 GHz,且最低反射损耗为-38.27 dB。Al₂O₃/SiC复合材料孔道内的Al₂O₃与SiC晶须交缠,形成大量电偶极矩,产生介电损耗;MoSi₂/SiC复合材料除介电损耗外还存在电阻损耗,使得复合材料电磁损耗增加,是较有前途的结构功能吸波材料。     

Design and fabrication of Al2O3f/SiCN composite with excellent microwave absorbing and mechanical properties

A new kind of structural and functional integration ceramic matrix composite material was prepared from high-performance alumina (Al₂O₃) fibers and absorbing silicon carbonitride (SiCN) ceramics via a combination of polymer infiltration pyrolysis (PIP) and chemical vapor infiltration (CVI) methods. The Al₂O₃ fiber annealed at its cracked temperature had enhanced permittivity, because the sizing agent on the Al₂O₃ fiber surface was cracked into pyrolysis carbon. For PIP + CVI Al₂O_3f/SiCN composites, PIP SiCN matrix with low conductivity was used as the matching phase, while CVI SiCN matrix with medium permittivity and dielectric loss was regarded as the reinforcing phase distributed in porous PIP SiCN matrix and inter-bundles of Al₂O₃ fiber to improve their mechanical and microwave absorption properties. The fracture toughness and flexural strength of Al₂O_3f/SiCN composite were determined to be 9.4 ± 0.5 MPa m^1/2 and 279 ± 28 MPa, respectively. Based on the design principles for impedance matching, the Al₂O_3f/SiCN composites before and after oxidation were used as loss and impedance layers, respectively. It was found that the optimized composite had the lowest reflection coefficient (RC) of −70 dB and the effective absorption bandwidth covering the whole X-band. In conclusion, Al₂O_3f/SiCN composite can serve as a high-temperature structural material with excellent microwave absorption properties for aerospace applications.     

Bi2O2CO3/Fe3O4磁性复合物在环境污染治理领域中的应用

以Fe₃O₄纳米粒子和Bi₂O₂CO₃为原料,采用溶剂热法制备Bi₂O₂CO₃/Fe₃O₄磁性复合物,并通过对印染废水中染料的去除、剩余污泥厌氧消化过程中产甲烷潜力的影响两方面探讨其在环境污染治理中的应用。借助X射线衍射（XRD）、扫描电镜（SEM）、傅里叶红外光谱（FTIR）和比表面积及孔径分析对Bi₂O₂CO₃/Fe₃O₄复合物进行表征分析,SEM分析结果表明复合物表面较粗糙,BET结果显示复合物的比表面积为9.2294m²/g,Fe₃O₄的引入大幅度增加了Bi₂O₂CO₃的比表面积,使其具有明显的介孔结构。一方面,以甲基橙（MO）为目标污染物,研究了不同实验条件下该材料对染料的去除效果,结果表明,最大吸附量可达14.373mg/g,且该吸附反应过程符合拟二级动力学和Langmuir吸附等温模型,趋于单分子层吸附;另一方面,评估了复合物对污泥厌氧消化产甲烷潜力的影响,结果表明,复合物的引入对污泥厌氧消化产甲烷过程有一定的促进作用,累积产甲烷量相比于对照组提高了10%。分别用一级动力学模型和修正Gompertz模型模拟厌氧消化过程,模拟结果显示一级动力学模型可以更好地描述引入Bi₂O₂CO₃/Fe₃O₄磁性复合物的污泥厌氧消化过程。